Method for producing dehydroepiandrosterone

A technology of dehydroepiandrosterone and production method, applied in the directions of steroids, organic chemistry, etc., can solve the problems of violent reaction, burns, fast hydrolysis reaction speed, etc., achieve stable chemical reaction, reduce production cost, and improve competitiveness Effect

Inactive Publication Date: 2009-02-11
HUBEI DANAO PHARMA CO LTD
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Problems solved by technology

The existing production method is: after the raw material is subjected to ketoxime reaction, then undergoes hydrolysis reaction, and finally refined (filtered, crystallized, centrifuged, dried) to obtain the finished product. The products produced all the time have "three lows and one yellow ", that is, low melting point, low content, low yield, and yellow color. The analysis reason is that the alkalinity of sodium hydroxide in the hydrolysis reaction is strong, and it is a strong electrolyte. The hydrolysis reaction speed is fast, the reaction is violent, and a large amount of heat is released. The heat is not taken away by the cooling medium, and the product is "burned", thereby generating new organic impurities, resulting in the above-mentioned shortcomings of the product

Method used

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Examples

Experimental program
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Effect test

Embodiment Construction

[0009] 1. Ketoxime reaction:

[0010] With ethanol 250kg (≥ 95%), pyridine 36kg (≥ 98%), pump in the tank, add hydroxylamine hydrochloride 13kg (≥ 98%), open steam and heat up 40-50 ℃, then dienolone acetate 60kg ( content ≥ 98%) was added, refluxed for 3.5 hours, cooled to 5°C, centrifuged and washed until neutral to obtain the required ketoxime.

[0011] 2. Bayesian reaction:

[0012] Put 360g of pure benzene (≥98%) and 30g of pyridine (≥98%) into the tank, raise the temperature to 40-50°C, then add the ketoxime reacted in the first step, and raise the temperature to 60°C, after the materials are completely dissolved, Cool down to 8°C, start dropping 30kg of phosphorus oxychloride (content ≥ 98%), the temperature in the tank is ≤ 16°C, finish dropping in 1.5 hours, keep warm for 3 hours, then add 90kg of hydrochloric acid solution dropwise, the content of hydrochloric acid is ≥ 30 %, the temperature in the tank is less than or equal to 25°C, after the dropwise addition is ...

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PUM

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Abstract

The invention discloses a production method for dehydroisoandrosterone, which comprises the steps of ketoxime reaction, Bering reaction, hydrolysis reaction, and obtaining a finished product after refining and is characterized in that: in the hydrolysis reaction, potassium carbonate and methanol are used for reacting with a Bering reactant; filtering, crystallization, centrifugalization and drying are carried out to the solution after reaction, thus obtaining the finished product. In the hydrolysis reaction, since the alkalinity of the potassium carbonate is moderate, the reaction has relatively slow speed, stable chemical reaction and little produced heat and is safe. After refining, the melting point, the content and the yield of the product are respectively increased by 2 DEG C, 1.5 percent and 3.4 percent; the color and luster and the appearance of the product are improved; various indexes of the product are placed in the front ranks of the same industry in China; the method is also proved to have safety, effectiveness and quality controllability; meanwhile, the method increases output and lowers production cost, the product quality not only meets the requirements of customers but also increases market competitive power.

Description

technical field [0001] The present invention relates to the production method of dehydroepiandrosterone. Background technique [0002] The molecular formula of dehydroepiandrosterone is: C 19 h 28 o 2 . The existing production method is: after the raw material is subjected to ketoxime reaction, then undergoes hydrolysis reaction, and finally refined (filtered, crystallized, centrifuged, dried) to obtain the finished product. The products produced all the time have "three lows and one yellow ", that is, low melting point, low content, low yield, and yellow color. The analysis reason is that the alkalinity of sodium hydroxide in the hydrolysis reaction is strong, and it is a strong electrolyte. The hydrolysis reaction speed is fast, the reaction is violent, and a large amount of heat is released. The heat is not taken away by the cooling medium, and the product is "burned", thereby generating new organic impurities, resulting in the above-mentioned shortcomings of the prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J1/00
Inventor 张良李元如
Owner HUBEI DANAO PHARMA CO LTD
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